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RWV nr. : RWV-011-120-059/04 Page nr. : 0 Document : Operation Manual Tousimis CPD Epcode : R59 Chapter : Table of contents Administrator : Documents Administrator TFF Date : 16-01-2008

Author: P.P.J. van Eerd

0. Table of contents 0. Table of contents .............................................................................................................. 0 1. Changes compared to previous versions .......................................................................... 1 2. Safety................................................................................................................................ 2

2.1 General ....................................................................................................................... 2 2.2 Chemicals ................................................................................................................... 2

3. General information ......................................................................................................... 3 4. Operation manual ............................................................................................................. 4

4.1 General ....................................................................................................................... 4 4.2 Operating Procedure ................................................................................................... 4

5. Process regulation .......................................................................................................... 12 5.1 Leak Correction Protocol ......................................................................................... 12 5.2 Errors during processing........................................................................................... 15

6. Instruction and test ......................................................................................................... 16

© Philips Research - DTS Company Restricted r59.doc

RWV nr. : RWV-011-120-059/04 Page nr. : 1 Document : Operation Manual Tousimis CPD Epcode : R59 Chapter : 1. Changes compared to previous versions Administrator : Documents Administrator TFF Date : 16-01-2008

1. Changes compared to previous versions Date Page

number New ver-sion num-ber

Description

30-07-2007 /01 First version with RWV number

31-07-2007 4 /02 Added text to check bottle weight in operating procedure

26-09-2007 4 & 13 /03 Changed necessary rest weight of bottle + procedure to put mode back from manual to automatic

16-01-2008 5, 6 /04 Added text & picture cleaning all process chamber parts preventing CO2 leakage during processing.


RWV nr. : RWV-011-120-059/04 Page nr. : 2 Document : Operation Manual Tousimis CPD Epcode : R59 Chapter : 2. Safety Administrator : Documents Administrator TFF Date : 16-01-2008

2. Safety

2.1 General The Tousimis Automegasamdri®-916B critical point dryer (CPD) uses isopropanol (IPA) and liquid CO2 (under pressure) for its drying processes. The liquid CO2 is stored in a bottle in a gas-cabinet in the grey area behind the CPD (CR2-M04) Only trained personnel are allowed to change the liquid CO2 bottle or to perform mainte-nance. Always make sure that all the necessary protective measures are taken care of when performing maintenance on the tool.

2.2 Chemicals Table 1: Chemicals that are being used in the Tousimis CPD

Formula Name Dangers C3H8O Isopropanol Highly Flammable, Irritating CO2 (l) Liquid carbon dioxide Stored under high pressure

(56 bar) Detailed information about these chemicals can be found in the corresponding Material Safety Data Sheets (MSDS).


RWV nr. : RWV-011-120-059/04 Page nr. : 3 Document : Operation Manual Tousimis CPD Epcode : R56 Chapter : 3. General information Administrator : Documents Administrator TFF Date : 16-01-2008

3. General information To avoid capillary forces causing a problem during drying free standing structures, the best method is to completely prevent them from occurring. One way of doing this is by critical point drying. Here the liquid is taken to supercritical state without passing the liquid-vapor boundary, thus avoiding sticking (see figure 1).

Figure 1: P-T graph for supercritical drying To achieve the sample is immersed in an alcohol (acetone, IPA, Ethanol etc.). The next step is to gradually replace the alcohol by a liquid which is capable of reaching the supercritical state within physically reachable values, e.g. liquid CO2. Next this liquid is brought into the super-critical state, for CO2 this means bringing the temperature above 31ºC and simultaneously to pressure above 1072 psi. After the CO2 reached the supercritical state and the reactor chamber can be vented slowly. Not too fast, because in that case the temperature drops too quickly resulting in the CO2 crossing the liquid-vapor boundary. The Tousimis Automegasamdri®-916B is a critical point dryer capable of drying 5 substrates in one run varying in size between 1cm x 1cm up to 8 inch in diameter. It uses liquid CO2 to replace the intermediate in which the substrates are immersed, in this case isopropanol.


RWV nr. : RWV-011-120-059/04 Page nr. : 4 Document : Operation Manual Tousimis CPD Epcode : R59 Chapter : 4. Operation manual Administrator : Documents Administrator TFF Date : 16-01-2008

4. Operation manual

4.1 General • The apparatus is flat independent. • In the holders the substrates should be placed faced-up on top of Teflon ring. • Always wear protective gloves.

4.2 Operating Procedure

1. Check the weight of the liquid CO2 bottle in the grey area of the cleanroom (CR2-M04). Whenever there is a chance that the weight will drop below 10,0 kg during processing, call the equipment-owner or back-up for a bottle change.

2. Turn “Chiller Power” ON at least 30 minutes prior to 1st run of the day. This is necessary to “Chill” coolant fluid to proper operating temperature required to cool chamber.

3. Turn “Condenser Power” ON



4. Turn “Chamber Power” ON

Green LED on VENT button will illuminate. This indicates the power is ON and the unit is standing by in the VENT mode.

5. Let the Tousimis CPD stand for 3-5 minutes. This initial wait period will allow all inter-

nally heated plumbing compo0nents to “warm-up”

6. The pressure gauge should be in the “0 psi” range.

Remove the chamber lid and carefully place lid up-side-down on a soft surface in prepara-tion for a process run. Once the chamber lid is removed, always protect chamber face.

7. Before processing thoroughly clean ALL process chamber parts with a whipping cloth and IPA. This means cleaning the chamber lid, the inside of the process chamber, the basket and spacer-ring(s), the stainless steel area around the bolts, and last but not least the cham-



ber O-ring as well as the backing ring (see picture) and the chamber gland.

NOTE: After every 10th run these two rings will be replaced to prevent CO2 leakage dur-ing processing. Therefore, after every 10th run contact the equipment owner or back-up to replace these two rings.

8. Now press the VENT button once. The VENT LED will begin to blink indicating the Tousimis CPD is in STANDBY mode. This indicates that the VENT solenoid is closed and you may now introduce IPA into the chamber.



9. Determine what size substrate you have and place the appropriate number of inserts into the chamber if required. At this point, you may fill the chamber with sufficient IPA to cover your substrates upon transfer.

NEVER EXPOSE CHAMBER TO ANY ACIDS

10. Carefully and quickly transfer your substrates into the Tousimis CPD process chamber using the specially designed baskets. Make sure that the substrates are placed faced-up and always on top of a Teflon ring. For best results, minimize the exposure time to air!

11. Carefully lower the chamber lid onto the chamber. Use fingers to evenly tighten the 10-knurled nuts around the circumference of the chamber lid. Then use the spanning wrench provided, to uniformly tighten each knurl nut in a “Star Pattern”. Tighten the knurl nuts in the numbered sequence as shown in the photo and on the lid itself. Repeat this rotation “Star Pattern” sequence at least 3 times, until the knurl nuts are unable to tighten further.

12. Once the chamber lid is secured, it is time to set the PURGE timer located on the right of

the push button switches. The “Purge Time” setting is best determined by the individual investigator. Some general “Purge Settings” are listed below: - To purge ¼ chamber full of IPA = 15 minute purge time - To purge ½ chamber full of IPA = 20 minute purge time



13. After the “Chill Power” has been ON for a minimum of 30 minutes, a process run may begin. Press the COOL button. The COOL LED will go ON, and the VENT LED will turn off. The chamber temperature will slowly begin to drop. The chamber will cool from the current temperature to ≤10ºC (cool time from 22ºC to 8ºC is about 8 minutes). Once the chamber reaches 10ºC, you may proceed to the next step.

14. Press the FILL button and the Tousimis CPD chamber will begin to fill with LCO2. From

this point forward, the Tousimis CPD will automatically cycle through all the drying se-quence modes until process completion. During the FILL mode, LCO2 will enter and fill the chamber for 8 minutes. If during the FILL mode a leak in the chamber is detected please proceed to §5.1. The process chamber temperature is automatically maintained be-low 10ºC during this FILL mode. The FILL rate is factory pre-set, but can be tuned for fragile structures.

15. After the 8 minute FILL mode expires, the Tousimis CPD will automatically advance into

the PURGE mode. This will be indicated by the illumination of the PURGE LED.

16. At this point of the cycle, the Tousimis CPD will remain in the PURGE mode for the du-

ration of the pre-set by the operator via the PURGE TIMER (see page 6). The IPA coming out of the Tousimis CPD Chamber Exhaust connect hose will be collected directly into the internal SOTER® Condenser. The process chamber temperature is automatically main-tained below 10ºC during this PURGE mode.

17. Upon completion of the PURGE mode, the Tousimis CPD will automatically advance into the POST-PURGE-FILL mode in which the chamber fills with LCO2 for an additional 4 minutes. This mode is indicated by both the FILL and PURGE LED’s simultaneous illu-mination. This mode helps to insure that the process chamber is full of LCO2 prior to ad-



vancing to the next mode.

18. Upon completion of the POST-PURGE-FILL mode, the PURGE and FILL LED’s will

turn off and the HEAT LED will illuminate. The HEAT mode is the stage in which the substrate(s) are carried through the “Critical Point”. Both the pressure and the temperature will steadily rise and be maintained above 1072 psi and 31ºC.

19. The chamber pressure will increase and go beyond 1072 psi, and will stabilize in the range

of 1350 psi (± 5%). As the temperature reaches 31ºC, the unit has achieved the “critical point” and this is where the ‘tousimis equilibrium1’ cycle starts. The HEAT LED will be-gin to blink for the next 4 minutes indicating the Tousimis CPD is in the ‘tousimis equilib-rium’.

It is normal for the temperature to stay above 31ºC during HEAT and BLEED modes

20. At the end of the 4 minute ‘tousimis equilibrium’ period, the Tousimis CPD will auto-matically advance into the BLEED mode. The HEAT LED will stop blinking and the BLEED LED will illuminate

21. At this point, the process chamber will begin to BLEED internal chamber pressure at an

average rate of 100 – 150 psi/min. The BLEED rate has been factory pre-set at 135 scfh (see flow-meter on the side of the cabinet), but can be tuned for fragile structures.

22. At approximately 360 psi, the Tousimis CPD will automatically advance from the BLEED mode into the VENT mode. The BLEED LED will turn off, while the VENT LED will il-

1 ‘Tousimis equilibrium’ is the point during the critical point passage in which both the pressure and temperature are maintained above the critical point for a period of 4 minutes prior to advancing into the BLEED mode.



luminate. The chamber pressure will then more rapidly drop back towards “0” psi.

23. It is not necessary to readjust the PURGE-VENT metering valve flow rate. The chamber

should then come to atmospheric pressure in approximately 4 minutes.

24. At this point, the chamber lid may be removed by alternatively and evenly loosening all of the knurl nuts using the spanning wrench in a “reverse star pattern”.

25. After loosening the lid, carefully remove the lid from the chamber and place the lid up-

side-down on a soft surface.

26. The substrates can then be removed from the chamber and further processed. After remov-ing the substrates, it is best to store the chamber lid back onto the chamber for protection. Seal the chamber with the lid to help keep it clean and moisture free.

27. After the final process run is complete for the day, power down the Tousimis CPD in the following sequence (see next page):



“Chiller Power OFF” → “Condenser Power OFF” → “Chamber Power OFF”


RWV nr. : RWV-011-120-059/04 Page nr. : 12 Document : Operation Manual Tousimis CPD Epcode : R59 Chapter : 5. Process regulation Administrator : Documents Administrator TFF Date : 16-01-2008

5. Process regulation

5.1 Leak Correction Protocol

1. If a chamber leak is detected during the initial FILL mode, it will typically be noticed be-tween the 400–600 psi range.

2. Turn OFF the “Chamber Power” Switch located on the Top Panel of the Tousimis CPD.

This will isolate the chamber and prevent any liquids from coming in or out of the cham-ber by immediately closing down all solenoids.

3. Wait 10 seconds in the OFF position and then simultaneously push the “BLEED” switch

for 10 seconds while turning “Chamber Power” switch ON as shown below. This is how the Tousimis CPD can be placed into a “Manual Mode” of operation.



4. Hold finger on BLEED switch for 10 seconds

5. Release the BLEED switch and press again

6. Now the Tousimis CPD is in the “Manual Mode”. You may open the BLEED meter valve

to accelerate the decrease in chamber pressure to “0” psi. This decreases the wait prior to opening the chamber lid by allowing chamber pressure to decrease at a faster rate. After completion turn the BLEED meter valve to its original value.



7. Carefully remove the chamber lid form the chamber. It is normal to see little bubbles in the intermediate fluid (IPA). This is due to carbonization.

NOTE: If necessary notify the equipment owner of back-up for inspection of the cham-ber O-ring.

8. Remember to reset the BLEED metering valve to its original Pre-Set position. Check value written on the Automegasamdri®-916B.

9. Turn Chamber Power Switch “OFF”. This will take the Automegasamdri®-916B back out of the “Manual Mode”.

10. Wait 10 seconds prior to turning Chamber Power Switch back “ON”. This will power the

Automegasamdri®-916B back up into the normal “Auto Mode” of operation by default



11. The VENT switch LED will illuminate as per normal start-up condition

12. Press the VENT switch once as soon as the VENT LED is illuminates when the power is

turned ON. This will initiate the VENT LED to blink, ON and OFF. This is the “Standby Mode” prior to initiating a run.

13. Either remove the substrates, carefully lower the lid onto the chamber and seal it with the

knurl nuts. Or if you wish to perform with another run leave the substrates in the chamber, fill the chamber with IPA and proceed with step 10 at page 6.

5.2 Errors during processing Whenever there are ERRORS or uncertainties occurring during processing of substrates, please contact the machine owner or back-up. Equipment ERRORS are made visual by simul-taneously blinking of all the LED’s of the push buttons.


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6. Instruction and test The only person, who is allowed to carry out the instruction, is the equipment owner. Nor-mally the instruction will take about half an hour and will be given only after reading this manual. First the major parts and possibilities of the machine will be explained with respect to running different substrate sizes. After this the complete operating screen and the correct way to run a cleaning process will be explained on the basis of the Operating Manual as described in chapter 4. Subsequently the student will perform a complete sequence of setting and running the correct drying process based upon a substrate of its/her own, independently as a test.
